Validation of an Analytical Method by Headspace Gas Chromatography with Flame Ionization and Evaluation of Matrix Effect of Volatile Compounds in Cat Food

Carvalho, Bruno M.; Santos, Patrícia D. S. dos; Silva, Geovane A. R. da; Senes, Carlos E. R.; Visentainer, Jesuí V.; Santos, Oscar O.

doi:10.21577/0103-5053.20230026

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Article • J. Braz. Chem. Soc. 34 (8) • Aug 2023 • https://doi.org/10.21577/0103-5053.20230026 copy

Validation of an Analytical Method by Headspace Gas Chromatography with Flame Ionization and Evaluation of Matrix Effect of Volatile Compounds in Cat Food

Authorship SCIMAGO INSTITUTIONS RANKINGS

This study describes the validation of a headspace gas chromatography with flame ionization (HS-GC-FID) method for the determination of propanal, pentanal, hexanal, octanal, and trans-2-nonenal originated by lipid oxidation from cat food samples, as well as the evaluation of the matrix effect in the results. This method was applied to the analysis of commercial cat food and proved to be suitable for the determination of these volatile compounds in different samples. Mean recoveries between 88 and 109% were obtained and repeatability expressed as relative standard deviation was always lower than 6.95%. The intra- and inter-assay precisions ranged from 0.44 to 20.88% and from 0.45 to 20.52%, respectively. In addition, the matrix effect of cat food samples was determined by comparing the slopes of the standard addition method, and the external calibration curve and its influences were verified. These results highlight the high potential of this method, which allows the determination of lipid oxidation products in cat food samples directly, without requiring prior sample preparation techniques.

Keywords:
aldehydes; lipid oxidation; cat food; degradation products; GC-FID

Factor	Level
Factor	-α	-1	0	+1	+α
Incubation temperature, A / °C	75	80	85	90	95
Incubation time, B / s	10	20	30	40	50
Salting out, C / (mol L^-1)	0.50	1	1.50	2	2.50
Water volume, D / mL	3.50	4	4.50	5	5.50

	Linear range / (µg g^-1)	Linear regression (y = ax + b)	Correlation coefficient (R)
Propanal	0.49-19.57	y = 2682x – 178.1	0.999
Pentanal	0.49-19.57	y = 375151.9x – 15036.5	0.999
Hexanal	0.49-19.57	y = 767.4x – 2.57	0.999
Octanal	0.49-19.57	y = 501.5x – 22.07	0.999
trans-2-Nonenal	0.49-19.57	y = 484.9x + 0.877	0.999

	Test	LOD / (µg g^-1)	Square sum	F-value
Propanal	intercept equality	1	87177400947.2153	126135.1328
	parallelism	1	24176310302.5149	34980.1907
	coincidence	2	92857419906.7263	67176.7159
Pentanal	intercept equality	1	199390504245679	18595.8186
	parallelism	1	6397360305403.83	596.639
	coincidence	2	310557992159161	14481.8333
Hexanal	intercept equality	1	675941508.5847	36750.5284
	parallelism	1	9775305.3598	531.4774
	coincidence	2	1141519997.9883	31031.8738
Octanal	intercept equality	1	983033594.4706	166614.3983
	parallelism	1	148870773.7869	25232.1127
	coincidence	2	1181792204.7842	100151.0011
trans-2-Nonenal	intercept equality	1	2199666806.2621	153519.9354
	parallelism	1	553314110.2871	38617.097
	coincidence	2	2385568676.0299	83247.2327

Compound	Level^a a n = 3; RSD: relative standard deviation. / (µg g^-1)	Recovery / %	RSD / %
Propanal	0.49	96-105	3.9
	4.89	98-103	1.94
	19.57	100-102	1.25
Pentanal	0.49	103-109	2.33
	4.89	97-102	1.76
	19.57	103-107	1.99
Hexanal	0.49	93-100	3.01
	4.89	98-103	1.61
	19.57	89-102	6.95
Octanal	0.49	88-97	3.82
	4.90	99-100	0.87
	19.60	95-101	2.63
trans-2-Nonenal	0.49	98-104	2.25
	4.89	98-101	1.35
	19.57	95-98	1.22

Sample	Propanal / (µg g^-1)	Hexanal / (µg g^-1)	Octanal / (µg g^-1)
1	0.54	0.68	0.77
2	0.56	0.70	0.77
3	0.59	0.71	0.70
4	0.65	0.79	0.70
5	0.56	0.81	0.75
6	0.59	0.79	0.70
RSD / %	6.65	7.51	4.85

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Propanal	Intra-day^a				Inter-days^b
	Day 1		Day 2		Inter-days^b
	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %
	0.47 ± 0.01^c	1.49	0.51 ± 0.01^c	1.18	0.49 ± 0.02^c	3.93
	2.94 ± 0.07^d	2.43	2.94 ± 0.01^d	0.37	2.94 ± 0.06^d	1.94
	20.05 ± 0.1^e	0.03	19.60 ± 0.41^e	0.41	19.82 ± 0.25^e	1.25
Pentanal	Intra-day				Inter-days
	Day 1		Day 2		Inter-days
	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %
	0.51 ± 0.00^c	0.80	0.53 ± 0.01^c	1.10	0.52 ± 0.01^c	2.33
	2.94 ± 0.08^d	2.76	2.94 ± 0.01^d	0.37	2.94 ± 0.05^d	1.76
	20.16 ± 0.01^e	0.03	20.88 ± 0.13^e	0.64	20.52 ± 0.41^e	1.99
Hexanal	Intra-day				Inter-days
	Day 1		Day 2		Inter-days
	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %
	0.49 ± 0.00^c	0.57	0.47 ± 0.01^c	3.01	0.48 ± 0.01^c	3.00
	2.94 ± 0.02^d	0.59	2.94 ± 0.07^d	2.49	2.94 ± 0.05^d	1.62
	19.73 ± 0.16^e	0.81	17.38 ± 0.08^e	0.46	18.55 ± 1.297^e	6.95
Octanal	Intra-day				Inter-days
	Day 1		Day 2		Inter-days
	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %
	0.47 ± 0.01^c	1.62	0.44 ± 0.01^c	1.45	0.45 ± 0.02^c	3.82
	2.94 ± 0.04^d	1.28	2.94 ± 0.01^d	0.50	2.94 ± 0.03^d	0.87
	19.71 ± 0.13^e	0.67	18.87 ± 0.29^e	1.55	19.29 ± 0.51^e	2.63
trans-2-Nonenal	Intra-day				Inter-days
	Day 1		Day 2		Inter-days
	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %	Average concentration / (µg g^-1)	RSD / %
	0.49 ± 0.00^c	0.41	0.49 ± 0.02^c	3.47	0.49 ± 0.01^c	2.25
	2.94 ± 0.03^d	1.11	2.94 ± 0.05^d	1.82	2.94 ± 0.04^d	1.35
	18.69 ± 0.14^e	0.77	18.84 ± 0.30^e	1.61	18.77 ± 0.23^e	1.22